Determination of trace level chemical warfare agents in water and slurry samples using hollow fibre-protected liquid-phase microextraction followed by gas chromatography-mass spectrometry
hollow fibre;
liquid-phase microextraction;
chemical warfare agents;
gas chromatography-mass spectrometry;
D O I:
10.1016/j.chroma.2006.05.030
中图分类号:
Q5 [生物化学];
学科分类号:
071010 ;
081704 ;
摘要:
A simple and solvent-minimised sample preparation technique based on hollow fibre-protected liquid-phase microextraction was investigated for the gas chromatography/mass spectrometric analysis of chemical warfare agents in water and slurry samples. The chemical warfare agents included four nerve agents and a blister agent. Parameters such as extraction solvent, salt concentration, stirring speed and extraction time were optimised using spiked deionised water samples. The technique provided a linear range of two orders of magnitude, good repeatability (RSDs < 10%, n = 6), good linearity (r(2) >= 0.995) and limits of detection (LODs) in the range of 0.02-0.09 mu g l(-1) (S/N = 3) under full scan mode. The optimised technique was also applied to more complex slurry samples and similar precision (RSD < 15%, n = 3) and limits of detection (0.02-0.2 mu g l(-1), S/N = 3) were obtained. (c) 2006 Elsevier B.V. All rights reserved.
机构:
Univ Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
de Almeida, Rafael Menck
de Lima, Diogenes Saulo
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Univ Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
de Lima, Diogenes Saulo
Seulin, Saskia Carolina
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Univ Sao Paulo, Fac Med, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
Seulin, Saskia Carolina
Leyton, Vilma
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Univ Sao Paulo, Fac Med, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
Leyton, Vilma
Pasqualucci, Carlos Augusto
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Univ Sao Paulo, Fac Med, BR-05508 Sao Paulo, Brazil
Univ Sao Paulo, Death Verificat Serv, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
Pasqualucci, Carlos Augusto
Munoz, Daniel Romero
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Univ Sao Paulo, Fac Med, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
Munoz, Daniel Romero
Osselton, Michael David
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Bournemouth Univ, Dept Forens & Biol Sci, Poole BH12 5BB, Dorset, EnglandUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil
Osselton, Michael David
Yonamine, Mauricio
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Univ Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, BrazilUniv Sao Paulo, Fac Pharmaceut Sci, BR-05508 Sao Paulo, Brazil